CN101891994A - Preparation method of heat resistant acetal wire enamel - Google Patents
Preparation method of heat resistant acetal wire enamel Download PDFInfo
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- CN101891994A CN101891994A CN2010102146921A CN201010214692A CN101891994A CN 101891994 A CN101891994 A CN 101891994A CN 2010102146921 A CN2010102146921 A CN 2010102146921A CN 201010214692 A CN201010214692 A CN 201010214692A CN 101891994 A CN101891994 A CN 101891994A
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Abstract
The invention relates to acetal wire enamel meeting the heat level of 155 DEG C and above, which has good coating film and conductor adhesion. The heat resistant acetal wire enamel comprises the following components: 280-310 parts of methylphenol, 390-450 parts of dimethylbenzene, 100-160 parts of butanol, 100-125 parts of polyvinyl acetal resins, 57-65 parts of novolac epoxy resins, 28-34 parts of organic silicon resins, 4-7 parts of melamine resins and 0.08-0.15 of leveling agents by mole. The method has the following advantages: 1. in the subsequent wire enamel baking process, the process is easy to control, the molecular weight is uniform and the consistency is good; 2. the peculiar smell generated under normal temperature and during baking is reduced; 3. the product is stable in storage; 4. the coating processability is good and the prepared product has bright, clean and uniform surface; and 5. the heat resistance class of the prepared product is not less than 155 DEG C (F class), the hot stamping temperature thereof is not less than 180 DEG C and the cut-through temperature thereof is not less than 240 DEG C; and the prepared product has excellent medium resistance and excellent adhesion.
Description
Technical field
The present invention relates to a kind of preparation method of heat resistant acetal wire enamel, especially a kind of preparation method of heat resistant type acetal insullac.
Background technology
Acetal wire enamel is traditional insulating material that can be used for production oil immersion environment electrical material coil wire rod in the world.Because the singularity of the coiling machine course of processing requires wire rod to have splendid paint film tack, outstanding transformer oil resistant performance, and can be under ℃ condition of working temperature≤120 life-time service, be widely used in the coating of oil-filled transformer winding coil wire rod.
At present according to international IEC60317-18/19 standard, the thermal level of tradition acetal paint is located in 105 ℃ or 120 ℃, but because transformer progressively develops to high pressure or ultra-high voltage direction, traditional acetal paint (or finished product wire rod) has been difficult to satisfy more and more higher thermal level requirement.
According to present market the acetal paint characteristic of confession, have following open defect:
1, heat-resisting low, general≤120 ℃ (E level);
2, lacquer fluid viscosity (general 〉=3800mpa.s/30 ℃) bigger than normal, technology stability is poor, and batch fluctuation is big;
3, paint film and conductor adhesion are poor, can not satisfy service requirements, particularly season difference variation;
4, solvent formula does not take into full account operation, and the peculiar smell pungency is big, and environmental pollution is serious.
Summary of the invention
The objective of the invention is to overcome above deficiency, a kind of acetal wire enamel that satisfies 155 ℃ and above thermal level is provided, paint film and conductor adhesion are good, with the manufacturing of the coil wire rod that satisfies requirements at the higher level.
The object of the present invention is achieved like this:
Described heat resistant acetal wire enamel comprises following component: 280～310 parts in cresols, 390～450 parts of dimethylbenzene, 100～160 parts in butanols, 100～125 parts of polyvinyl acetal resins, 57～65 parts of novolac epoxys, 28～34 parts of silicone resins, 0.08～0.15 part of 4～7 parts of melamine resins and flow agent, described umber is molfraction.
As preferred version, the hydroxy radical content of described polyvinyl acetal resin is 9～13%, and acetoxyl group content 2～4%, molecular weight are 10000～20000.
As preferred version, the content of ortho-cresol is not more than 2% in the described cresols.
As preferred version, described novolac epoxy is an ortho-cresol formaldehyde Resins, epoxy, and oxirane value is 0.42～0.50, and preferred novolac epoxy is ECN704#.
As preferred version, described silicone resin is an epoxy modified silicone resin, and oxirane value is 0.01～0.03, and preferred silicone resin is ES-6.
As preferred version, described flow agent is polyether-modified polysiloxane, the BYK-300 that preferred Bi Ke chemical company produces.
Each components dissolved, physical mixed evenly can be obtained described heat resistant acetal wire enamel.According to the chemical reactivity of different components, preferably preparation as follows:
Step a, 240～260 parts in cresols, 310～360 parts of dimethylbenzene, butanols are mixed as solvent for 100～160 parts, when being heated to 50 ± 5 ℃, and employing progressively adds even feeding mode, in 0.5～1h, in solvent, drop into 100～125 parts of polyvinyl acetal resins, and insulated and stirred to polyvinyl acetal resin dissolves fully under 80 ± 5 ℃ of temperature, makes work in-process A;
Step b, with 40～50 parts in cresols, 80～90 parts of dimethylbenzene stir, and are heated to 50 ± 5 ℃, and add 57～65 parts of novolac epoxys, and insulated and stirred to novolac epoxy dissolves fully under 60 ± 5 ℃ of temperature, makes work in-process B;
Step c, work in-process A in the reactor is cooled to 50 ± 5 ℃, drop into the work in-process B that b set by step makes, stir, and then add 28～34 parts of silicone resins, 4～7 parts of melamine resins and 0.08～0.15 part of flow agent are stirred to melamine resin and dissolve fully, remove by filter impurity and obtain heat resistant acetal wire enamel.
Owing to adopted technique scheme, select for use the cresols that do not contain or contain ortho-cresol less, dimethylbenzene, butanols mixture as solvent, avoided the generation of solvent peculiar smell, give use good Technological adaptability, meet the RoHS of European Union environmental protection command request; Select for use the novolac epoxy of heat resistant type to cooperate, significantly improved resistance toheat and with the tack of conductor, have good intermiscibility between component, good product consistency, technological operation is easy, the yield rate height.Select for use melamine resin as the bridge formation linking agent, cure in the process at the subsequent packet lacquer, epoxide group in hydroxyl in melamine resin, the polyvinyl acetal resin and novolac epoxy and the epoxy modified silicone resin is cured reaction, reaction process is steady, no coupling product produces, make paint film have better oil resistance and physical strength, adopt suitable flow agent significantly to improve the coating flow leveling of this lacquer.The coating of product fine has been given in the cooperation of above component, with the bonds well tack of conductor, and higher heat-resisting, oil resistance.After testing, the environment protection type high-strength heat resistant acetal wire enamel product performance index made of the present invention is as follows:
1, outward appearance: light yellow to the transparent thick liquid of red-brown, there are not mechanical impurity and insoluble particle;
2, viscosity: 1.0～4.0pa.s (rotational viscosimeter/30 ± 1 ℃)
3, solids content: 12～22% (180 ℃/1-1.2g/1h)
The present invention has the following advantages:
1, the subsequent packet lacquer cures in the process, novolac epoxy and silicone resin and Derlin reaction, and process is controlled easily, and no coupling product produces, and molecular weight is even, and high conformity effectively improves thermotolerance;
2, adopt high-quality low odor solvent burden ratio, reduced normal temperature and when curing peculiar smell produce, system meets the RoHS of European Union standard-required;
3, product shelf-stable, through the time viscosity change for a short time, viscosity changes less than 10% * original viscosity (6 months);
4, adopt suitable flow agent, coating processes is good, and the finished product any surface finish is even;
5, finished product (is example with Φ 0.31mm) temperature classification 〉=155 ℃ (F level) that apply with this prescription lacquer, heat is dashed 〉=180 ℃, softens to puncture 〉=240 ℃; Media-resistant (transformer oil) excellent property (by the 1000h oil resistant test); Have excellent tack, the otch farad is stretched 15-20%≤1d, good stability; Mechanical property is strong.
Embodiment
In following examples,
The mass percentage content of ortho-cresol is in the cresols :≤2%;
Polyvinyl acetal resin: the clear and electric material in Tianjin company produces, and the trade mark: PVF, hydroxy radical content are 9.0～13.0%, and acetoxyl group content 2.0-4.0%, molecular weight are 95000～134000;
Resol: ECN704#, Nan Ya Plastics company in Taiwan produces;
Melamine resin: 582#, Jiangsu three lignify worker company limiteds produce;
Silicone resin: ES-6, the Wujiang resin company limited that makes a concerted effort produces;
Flow agent: BYK-300, Bi Ke chemical company produces.
In the Comparative Examples,
Industry cresols be neighbour// to cresols;
Polyvinyl acetal resin: the clear and electric material in Tianjin company limited produces, and the trade mark: PVF, hydroxy radical content are 9.0-13.0%, and acetoxyl group content 2.0-4.0%, molecular weight are 95000-134000;
Cresol Formaldehyde Resin: 2402#, Shanghai Resin Factory Co., Ltd. produces;
Melamine resin: 582#, Jiangsu three lignify worker company limiteds produce.
Below by embodiment the present invention is further described.
Embodiment 1:
In molar ratio, in the reactor that has agitator and return line, add 240 parts in cresols, 360 parts of dimethylbenzene, 100 parts in butanols, turn on agitator and heating are when treating that temperature reaches 50 ± 5 ℃, in 0.5～1 hour, adopting progressively, feed way drops into 125 parts of polyvinyl acetal resins in batches, and under 80 ± 5 ℃ of temperature insulated and stirred 3h, be cooled to 50 ± 5 ℃, make work in-process A; In molar ratio, in the reactor that has agitator and return line, add 40 parts in cresols, 86 parts of dimethylbenzene, turn on agitator and heating drop into 62 parts of novolac epoxys, are incubated 2h under 60 ± 5 ℃ of temperature, are cooled to 50 ± 5 ℃, make work in-process B; Work in-process B put among the work in-process A stir, and then add 28 parts, 4 parts melamine resins of silicone resin, insulation is at 50 ± 5 ℃/2h, until liquid clarification homogeneous, cool to less than 45 ℃, add 0.1 part of flow agent, stir 1h, filter and make finished product.
Embodiment 2:
In molar ratio, in the reactor that has agitator and return line, add 260 parts in cresols, 330 parts of dimethylbenzene, 120 parts in butanols, turn on agitator and heating are when treating that temperature reaches 50 ± 5 ℃, in 0.5～1 hour, adopting progressively, feed way drops into 100 parts of polyvinyl acetal resins in batches, and under 80 ± 5 ℃ of temperature insulated and stirred 3h, be cooled to 50 ± 5 ℃, make work in-process A; In molar ratio, in the reactor that has agitator and return line, add 50 parts in cresols, 90 parts of dimethylbenzene, turn on agitator and heating drop into 65 parts of novolac epoxys, are incubated 2h under 60 ± 5 ℃ of temperature, are cooled to 50 ± 5 ℃, make work in-process B; Work in-process B put among the work in-process A stir, and then add 34 parts, 7 parts melamine resins of silicone resin, insulation is at 50 ± 5 ℃/2h, until liquid clarification homogeneous, cool to less than 45 ℃, add 0.15 part of flow agent, stir 1h, filter and make finished product.
Embodiment 3:
In molar ratio, in the reactor that has agitator and return line, add 250 parts in cresols, 320 parts of dimethylbenzene, 140 parts in butanols, turn on agitator and heating are when treating that temperature reaches 50 ± 5 ℃, in 0.5～1 hour, adopting progressively, feed way drops into 105 parts of polyvinyl acetal resins in batches, and under 80 ± 5 ℃ of temperature insulated and stirred 3h, be cooled to 50 ± 5 ℃, make work in-process A; In molar ratio, in the reactor that has agitator and return line, add 45 parts in cresols, 85 parts of dimethylbenzene, turn on agitator and heating drop into 60 parts of novolac epoxys, are incubated 2h under 60 ± 5 ℃ of temperature, are cooled to 50 ± 5 ℃, make work in-process B; Work in-process B put among the work in-process A stir, and then add 32 parts, 6 parts melamine resins of silicone resin, insulation is at 50 ± 5 ℃/2h, until liquid clarification homogeneous, cool to less than 45 ℃, add 0.12 part of flow agent, stir 1h, filter and make finished product.
Embodiment 4:
In molar ratio, in the reactor that has agitator and return line, add 260 parts in cresols, 310 parts of dimethylbenzene, 160 parts in butanols, turn on agitator and heating are when treating that temperature reaches 50 ± 5 ℃, in 0.5～1 hour, adopting progressively, feed way drops into 110 parts of polyvinyl acetal resins in batches, and under 80 ± 5 ℃ of temperature insulated and stirred 3h, be cooled to 50 ± 5 ℃, make work in-process A; In molar ratio, in the reactor that has agitator and return line, add 48 parts in cresols, 82 parts of dimethylbenzene, turn on agitator and heating drop into 57 parts of novolac epoxys, are incubated 2h under 60 ± 5 ℃ of temperature, are cooled to 50 ± 5 ℃, make work in-process B; Work in-process B put among the work in-process A stir, and then add 30 parts, 5 parts melamine resins of silicone resin, insulation is at 50 ± 5 ℃/2h, until liquid clarification homogeneous, cool to less than 45 ℃, add 0.08 part of flow agent, stir 1h, filter and make finished product.
Comparative Examples
In molar ratio, in the reactor that has agitator and return line, add 145 parts in industrial cresols, 125 parts of dimethylbenzene, 510 parts in furfural, 72 parts of toluene stir and heating, slowly drop into 100 parts of polyvinyl acetals, be warmed up to 80～90 ℃ after adding, be incubated 2 hours, cool to 60 ± 5 ℃ after the dissolving fully, make work in-process.In molar ratio, drop into Cresol Formaldehyde Resin (2402# resol) 75 parts, melamine resin fully stirs under 60 ± 5 ℃ of temperature as (582# aminoresin) 6.3 parts, and dissolving is abundant, and cold filtration impurity makes finished product.
The testing performance index of the foregoing description and Comparative Examples gained heatproof acetal paint sees Table 1.
Claims (9)
1. heat resistant acetal wire enamel, it is characterized in that, comprise following component: 280～310 parts in cresols, 390～450 parts of dimethylbenzene, 100～160 parts in butanols, 100～125 parts of polyvinyl acetal resins, 57～65 parts of novolac epoxys, 28～34 parts of silicone resins, 0.08～0.15 part of 4～7 parts of melamine resins and flow agent, described umber is molfraction.
2. heat resistant acetal wire enamel as claimed in claim 1 is characterized in that, the hydroxy radical content of described polyvinyl acetal resin is 9～13%, and acetoxyl group content 2～4%, molecular weight are 95000～134000.
3. heat resistant acetal wire enamel as claimed in claim 1 is characterized in that the content of ortho-cresol is not more than 2% in the described cresols.
4. heat resistant acetal wire enamel as claimed in claim 1 is characterized in that, described novolac epoxy is an ortho-cresol formaldehyde Resins, epoxy, and oxirane value is 0.42～0.50.
5. heat resistant acetal wire enamel as claimed in claim 4 is characterized in that, described novolac epoxy is ECN704#.
6. heat resistant acetal wire enamel as claimed in claim 1 is characterized in that, described silicone resin is an epoxy modified silicone resin, and oxirane value is 0.01～0.03.
7. heat resistant acetal wire enamel as claimed in claim 7 is characterized in that, described silicone resin is ES-6.
8. heat resistant acetal wire enamel as claimed in claim 1 is characterized in that, described flow agent is polyether-modified polysiloxane.
9. as each described heat resistant acetal wire enamel among the claim 1-8, it is characterized in that described heat resistant acetal wire enamel prepares as follows:
Step a, 240～260 parts in cresols, 310～360 parts of dimethylbenzene, butanols are mixed as solvent for 100～160 parts, when being heated to 50 ± 5 ℃, and employing progressively adds even feeding mode, in 0.5～1h, in solvent, drop into 100～125 parts of polyvinyl acetal resins, and insulated and stirred to polyvinyl acetal resin dissolves fully under 80 ± 5 ℃ of temperature, makes work in-process A;
Step b, with 40～50 parts in cresols, 80～90 parts of dimethylbenzene stir, and are heated to 50 ± 5 ℃, and add 57～65 parts of novolac epoxys, and insulated and stirred to novolac epoxy dissolves fully under 60 ± 5 ℃ of temperature, makes work in-process B;
Step c, work in-process A in the reactor is cooled to 50 ± 5 ℃, drop into the work in-process B that b set by step makes, stir, and then add 28～34 parts of silicone resins, 4～7 parts of melamine resins and 0.08～0.15 part of flow agent are stirred to melamine resin and dissolve fully, remove by filter impurity and obtain heat resistant acetal wire enamel.
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| CN103013207A (en) * | 2012-12-12 | 2013-04-03 | 铜陵三佳变压器有限责任公司 | Heat-resistant epoxy resin paint |
| CN103122200A (en) * | 2013-03-06 | 2013-05-29 | 溧阳市佳禾电子材料有限公司 | Expoxy self-adhesion paint with heat dissipation function and preparation method thereof |
| CN103333562A (en) * | 2013-07-05 | 2013-10-02 | 苏州圣利线缆有限公司 | Acetal enamelled wire paint |
| CN103694885A (en) * | 2013-12-04 | 2014-04-02 | 铜陵三佳变压器有限责任公司 | Wire enamel modified by organic silicon resin and preparation method of wire enamel |
| CN103694860A (en) * | 2013-12-04 | 2014-04-02 | 铜陵三佳变压器有限责任公司 | Acetal wire enamel meeting thermal level of 155 DEG C and more for transformer and preparation method of acetal wire enamel |
| CN103725119A (en) * | 2013-12-06 | 2014-04-16 | 天津昭鑫电材科技有限公司 | PVF paint with high solid content and preparation method thereof |
| CN103725189A (en) * | 2013-11-25 | 2014-04-16 | 铜陵天河特种电磁线有限公司 | Formal wire enamel and preparation method thereof |
| CN103725056A (en) * | 2013-11-25 | 2014-04-16 | 铜陵天河特种电磁线有限公司 | Epoxy wire enamel and preparation method thereof |
| CN103725154A (en) * | 2013-11-25 | 2014-04-16 | 铜陵天河特种电磁线有限公司 | Organosilicon wire enamel with thermal level up to 155 DEG C or above and preparation method of organosilicon wire enamel |
| CN103725168A (en) * | 2013-11-25 | 2014-04-16 | 铜陵天河特种电磁线有限公司 | Acetal wire enamel and preparation method thereof |
| CN103725177A (en) * | 2013-11-25 | 2014-04-16 | 铜陵天河特种电磁线有限公司 | Modified aluminum nitride wire enamel and preparation method thereof |
| CN103740194A (en) * | 2013-12-06 | 2014-04-23 | 天津昭鑫电材科技有限公司 | Low viscosity polyvinyl formal (PVF) paint and production method thereof |
| CN103881642A (en) * | 2014-03-21 | 2014-06-25 | 溧阳市佳禾电子材料有限公司 | Coating glue with good binding feature for heat-resisting voice coil skeleton and preparation method of coating glue |
| CN104693919A (en) * | 2015-03-20 | 2015-06-10 | 溧阳市佳禾电子材料有限公司 | Polyvinyl acetal insulating paint and preparation method thereof |
| CN107129729A (en) * | 2017-05-26 | 2017-09-05 | 王成宜 | A kind of B grades of heat-proof polythene alcohol formal enamelled wire insulated paint and preparation method thereof |
| CN107129743A (en) * | 2017-06-07 | 2017-09-05 | 合肥励仙电力工程有限公司 | A kind of transformer heat-resisting anticorona varinish enamel and preparation method thereof |
| CN108376577A (en) * | 2018-03-15 | 2018-08-07 | 无锡统力电工股份有限公司 | PVF/B self-adhering transposed conductors and preparation method thereof |
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Application publication date: 20101124 |